z-1-[4-(2-Benzyloxyethoxy)-phenyl]-4-chloro-1,2-diphenyl-but-1-ene → Ospemifene

HRID 1416343ノート

反応式

HRID 1416343 の反応式
C([O:8][CH2:9][CH2:10][O:11][C:12]1[CH:17]=[CH:16][C:15](/[C:18](/[C:29]2[CH:34]=[CH:33][CH:32]=[CH:31][CH:30]=2)=[C:19](\[C:23]2[CH:28]=[CH:27][CH:26]=[CH:25][CH:24]=2)/[CH2:20][CH2:21][Cl:22])=[CH:14][CH:13]=1)C1C=CC=CC=1>C(OCC)(=O)C.C(O)C.[Pd]>[Cl:22][CH2:21][CH2:20]/[C:19](/[C:23]1[CH:24]=[CH:25][CH:26]=[CH:27][CH:28]=1)=[C:18](/[C:15]1[CH:14]=[CH:13][C:12]([O:11][CH2:10][CH2:9][OH:8])=[CH:17][CH:16]=1)\[C:29]1[CH:30]=[CH:31][CH:32]=[CH:33][CH:34]=1

参加物

5

反応物 1

HCID 70116950z-1-[4-(2-Benzyloxyethoxy)-phenyl]-4-chloro-1,2-diphenyl-but-1-ene

生成物 1

HCID 3036505Ospemifene

試薬・触媒・溶媒 3

HCID 23938Palladium触媒HCID 702Ethanol溶媒HCID 8857Ethyl Acetate溶媒

実験手順

Z-1-[4-(2-benzyloxyethoxy)-phenyl]-4-chloro-1,2-diphenyl-but-1-ene (36 g, 0.08 mol) was dissolved in the mixture of ethyl acetate (350 ml) and ethanol (350 ml). Palladium on carbon (5%, 0.28 g) was added and the solution was flushed with hydrogen gas until there was not any starting compound left (thin layer chromatography). Palladium on carbon was filtered off through siliceous earth and the filtrate was evaporated. The residue was crystallized from the mixture of ethanol (155 ml) and water (65 ml). Yield 20 g.

後処理

  1. customthe solution was flushed with hydrogen gas until there
  2. waitleft (thin layer chromatography)
  3. filtrationPalladium on carbon was filtered off through siliceous earth
  4. customthe filtrate was evaporated
  5. customThe residue was crystallized from the mixture of ethanol (155 ml) and water (65 ml)

出典と根拠

ORDレコード
ord-cf2d751911fd45c1a6d99deb14d0f845
出典データセット
uspto-grants-1999_06
特許番号
US05912273

反応ノート

読み込み中…